Epoxy silicone and process for producing same, and curable mix composition using same and use thereof

Active Publication Date: 2010-05-13
ASAHI KASEI CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0061]According to the present invention, it is possible to provide epoxy silicone having transparency, light resistance, heat resistance, heat discoloration resistance, crack resistance and adhesiveness, and suitable for use in a sealing material for a light-emitting device; a curable mix composition for sealing a light-emitting device, containing the epoxy silicone, and a light-emitting component such as light-emitting diode,

Problems solved by technology

Conventional compositions containing an epoxy resin, such as bisphenol A-based epoxy resin and bisphenol F-based epoxy resin, as a main component, actually do not have sufficient properties.
However, the epoxy silicone formed of a T structure as a main component is brittle and therefore, it is difficult to satisfy crack resistance required for a light-emitting device sealing m

Method used

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  • Epoxy silicone and process for producing same, and curable mix composition using same and use thereof
  • Epoxy silicone and process for producing same, and curable mix composition using same and use thereof
  • Epoxy silicone and process for producing same, and curable mix composition using same and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Example

Example 1

Production of [Epoxy Silicone-1a]

[0346]A 3 L reactor with a reflux condenser, a thermometer and a stirrer was purged with dry nitrogen. Under dry nitrogen conditions, the reactor was charged with 80 g of 1,3,5,7-tetramethylcyclotetrasiloxane (a reagent manufactured by Shin-Etsu Chemical Co., Ltd.) dehydrated, distillated and purified under dry nitrogen; 37.2 g of 1,3-divinyltetramethyldisiloxane (a reagent manufactured by Shin-Etsu Chemical Co., Ltd.) dehydrated, distillated and purified under dry nitrogen; 122.6 g of 4-vinylcyclohexcene oxide (a reagent manufactured by Aldrich) dehydrated, distillated and purified under dry nitrogen, and 925 g of 1,4-dioxane (a reagent manufactured by Wako Pure Chemical Industries Ltd.) dehydrated, distillated and purified under nitrogen. Thereafter, the mixture was heated in an oil bath increased to 70° C. while stirring under an atmospheric-pressure dry nitrogen atmosphere.

[0347]After the temperature of the interior solution exceeded 65°...

Example

Example 2

Production of [Epoxy Silicone-2a]

[0357]A 3 L reactor with a reflux condenser, a thermometer and a stirrer was purged with dry nitrogen. Under dry nitrogen conditions, the reactor was charged with 80 g of 1,3,5,7-tetramethylcyclotetrasiloxane (a reagent manufactured by Shin-Etsu Chemical Co., Ltd.) dehydrated, distillated and purified under dry nitrogen; 37.2 g of 1,3-divinyltetramethyldisiloxane (a reagent manufactured by Shin-Etsu Chemical Co., Ltd.) dehydrated, distillated and purified under dry nitrogen; 122.6 g of 4-vinylcyclohexcene oxide (a reagent manufactured by Aldrich) dehydrated, distillated and purified under dry nitrogen and 925 g of ethylene glycol dimethyl ether (a reagent manufactured by Aldrich). Thereafter, the mixture was heated in an oil bath increased to 83° C. while stirring under an atmospheric-pressure dry nitrogen atmosphere.

[0358]An ethylene glycol dimethyl ether solution (5.6 g) of a platinum divinyltetramethyldisilicone complex containing 500 ppm...

Example

Example 3

Production of [Epoxy Silicone-3a]

[0368][Epoxy silicone-3a] (195 g) reduced in low boiling-point compounds was obtained in the same manner as in Example 1 except that, in the hydrosilylation reaction, 1,3-divinyltetramethyldisiloxane (55.8 g) was used; 4-vinylcyclohexene oxide (97.6 g) was used; 1,4-dioxane (900 g) was used; the 1,4-dioxane solution (3.6 g) of a platinum divinyltetramethyldisilicone complex containing 500 ppm of platinum in terms of platinum element was used; and after the hydrosilylation reaction, the solution was cooled, and thereafter, acetonitrile (900 g) was added.

[0369]Immediately before termination of the hydrosilylation reaction, a sample was taken. As a result, the hydrosilylation reaction was found to proceed quantitatively and an unreacted SiH unit was not detected.

[0370]At the initiation of the reaction, the ratio (r2 / r1), which is the ratio of the total number of mole (r1) of the SiH unit of organohydrogensilicone to the number of mole (r2) of t...

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Abstract

An epoxy silicon, which comprises at least a compound represented by the following general formula (1), and a compound represented by the following general formula (2); and which is represented by an average composition formula (3), wherein a value of [g/(a+b+c+d+e+f+g+h+i+j)] falls within a range of 0.020 or less.

Description

TECHNICAL FIELD[0001]The present invention relates to epoxy silicone suitably used as a main component of a curable mix composition for use in light-emitting device sealing materials, lenses, and the like.BACKGROUND ART[0002]Conventionally, an epoxy resin composition using an acid anhydride-based hardening agent provides a transparent hardened material and has been suitably used as a sealing material for light-emitting devices having high heat resistance, such as light-emitting diodes and photodiodes. However, with recent development of high-performance optical semiconductors, a hardened material, which has not only good transparency and high heat resistance but also excellent light resistance, oxidation resistance and crack resistance at the time of a hot and cold cycle in accordance with the on / off cycle of an LED, has been required as a sealing resin. Conventional compositions containing an epoxy resin, such as bisphenol A-based epoxy resin and bisphenol F-based epoxy resin, as a...

Claims

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Application Information

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IPC IPC(8): C08L83/06C08G77/04
CPCC08G59/306C08G59/3254C08G77/14C08G77/38C08G77/50C08L63/00H01L2924/0002C08L83/06C08L83/14H01L23/296H01L2924/00C08G77/06G02B1/04
Inventor KURODA, YOSHITOYOKOYAMA, MASAKOODA, HIROJI
Owner ASAHI KASEI CHEM CORP
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